CN113376351B - Method for inspecting columnar honeycomb molded body before or after firing - Google Patents
Method for inspecting columnar honeycomb molded body before or after firing Download PDFInfo
- Publication number
- CN113376351B CN113376351B CN202011472609.0A CN202011472609A CN113376351B CN 113376351 B CN113376351 B CN 113376351B CN 202011472609 A CN202011472609 A CN 202011472609A CN 113376351 B CN113376351 B CN 113376351B
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- China
- Prior art keywords
- columnar honeycomb
- honeycomb molded
- molded body
- firing
- cells
- Prior art date
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- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
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- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06T—IMAGE DATA PROCESSING OR GENERATION, IN GENERAL
- G06T7/00—Image analysis
- G06T7/0002—Inspection of images, e.g. flaw detection
- G06T7/0004—Industrial image inspection
- G06T7/001—Industrial image inspection using an image reference approach
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06T—IMAGE DATA PROCESSING OR GENERATION, IN GENERAL
- G06T7/00—Image analysis
- G06T7/0002—Inspection of images, e.g. flaw detection
- G06T7/0004—Industrial image inspection
- G06T7/0006—Industrial image inspection using a design-rule based approach
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/22—Fuels; Explosives
- G01N33/222—Solid fuels, e.g. coal
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/88—Investigating the presence of flaws or contamination
- G01N21/8851—Scan or image signal processing specially adapted therefor, e.g. for scan signal adjustment, for detecting different kinds of defects, for compensating for structures, markings, edges
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/88—Investigating the presence of flaws or contamination
- G01N21/95—Investigating the presence of flaws or contamination characterised by the material or shape of the object to be examined
- G01N21/9515—Objects of complex shape, e.g. examined with use of a surface follower device
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06T—IMAGE DATA PROCESSING OR GENERATION, IN GENERAL
- G06T7/00—Image analysis
- G06T7/60—Analysis of geometric attributes
- G06T7/62—Analysis of geometric attributes of area, perimeter, diameter or volume
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/88—Investigating the presence of flaws or contamination
- G01N21/95—Investigating the presence of flaws or contamination characterised by the material or shape of the object to be examined
- G01N21/956—Inspecting patterns on the surface of objects
- G01N21/95692—Patterns showing hole parts, e.g. honeycomb filtering structures
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06T—IMAGE DATA PROCESSING OR GENERATION, IN GENERAL
- G06T2207/00—Indexing scheme for image analysis or image enhancement
- G06T2207/30—Subject of image; Context of image processing
- G06T2207/30108—Industrial image inspection
- G06T2207/30164—Workpiece; Machine component
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Computer Vision & Pattern Recognition (AREA)
- Theoretical Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Quality & Reliability (AREA)
- Geometry (AREA)
- Signal Processing (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- Filtering Materials (AREA)
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
- Processes For Solid Components From Exhaust (AREA)
Abstract
The invention provides a method for inspecting a columnar honeycomb formed body before or after firing, which can be performed in a nondestructive manner and can replace strength inspection. A method of inspecting a columnar honeycomb formed body before or after firing, the columnar honeycomb formed body having a columnar honeycomb structure portion including an outer peripheral side wall and partition walls disposed on an inner peripheral side of the outer peripheral side wall, the partition walls partitioning a plurality of cells forming flow paths from a first bottom surface to a second bottom surface, the method comprising: shooting at least one of the first bottom surface and the second bottom surface of the columnar honeycomb formed body before or after firing by using a camera, and generating an image of at least one of the first bottom surface and the second bottom surface; a step of measuring the sizes of the openings of the plurality of cells in the image; and a step of determining abnormal cells having openings with a size deviating from a predetermined allowable range from among the plurality of cells based on the measurement result of the size of the opening, and counting the number of abnormal cells.
Description
Technical Field
The invention relates to a method for inspecting columnar honeycomb molded bodies.
Background
In various fields such as automobiles, chemistry, electric power, and steel, ceramic columnar honeycomb structures excellent in heat resistance and corrosion resistance are used as catalyst carriers and filters used for environmental measures, recovery of specific materials, and the like. The columnar honeycomb structure has an outer peripheral side wall and partition walls which are disposed on the inner peripheral side of the outer peripheral side wall and which partition a plurality of cells extending from one bottom surface to the other bottom surface. Generally, a columnar honeycomb structure is produced by mixing and kneading ceramic raw material powder, a dispersion medium, a binder, a pore-forming agent, etc., forming a green body, molding the green body into a predetermined shape, and then firing the columnar honeycomb molded body to produce a columnar honeycomb structure.
The columnar honeycomb structure needs to have sufficient mechanical strength in order to withstand impact and thermal load. In particular, a columnar honeycomb structure used as a filter or a catalyst carrier for a vehicle must have sufficient mechanical strength to enable it to be disposed in a metal case in a process called "canning".
The 1 index of the mechanical strength of the columnar honeycomb structure is the isostatic fracture strength. In the measurement of the isostatic fracture strength of the columnar honeycomb structure, an experiment was performed in which the columnar honeycomb structure was immersed in water in a pressure vessel, and the water pressure was gradually increased to apply isotropic pressure to the columnar honeycomb structure. As the water pressure in the pressure vessel gradually increases, the partition walls or the outer peripheral side walls of the columnar honeycomb structure eventually break. The value of the pressure at which the failure occurred (failure strength) was the isostatic failure strength.
However, when the isostatic fracture strength is measured, a time is required to perform an operation of fixing the test article in the pressure vessel and applying pressure. In addition, the columnar honeycomb structure was damaged by measurement of the isostatic fracture strength. Therefore, it is not realistic to directly measure the isostatic fracture strength in order to examine the quality of the columnar honeycomb structure. In view of the above, a method of easily performing strength inspection of a columnar honeycomb structure has been proposed.
For example, JP-A2017-96879 (patent document 1) and JP-A2001-41867 (patent document 2) propose a simple breaking strength test method using an elastomer, which can shorten the measurement time.
Japanese patent application laid-open publication No. 2019-512079 (patent document 3) discloses a non-contact method for characterizing the isostatic fracture strength of a ceramic article, which includes the steps of: the method includes the steps of recording a digital image of a web for a ceramic article having the web, forming a 2D representation of the ceramic article based on the digital image, simulating a selected amount of isostatic pressure given by the 2D representation to determine a maximum stress value within the 2D representation of the web, and determining an isostatic failure strength of the ceramic article using the maximum stress value.
Further, although not an invention for the purpose of inspecting the strength of a columnar honeycomb structure, japanese patent application laid-open No. 2015-161543 (patent document 4) proposes a method for measuring the size of inscribed circles inscribed in partition walls for only a predetermined part of cells by using an image analysis device for the purpose of inspecting cell deformation defects of a ceramic honeycomb structure in a short time.
Prior art literature
Patent literature
Patent document 1: japanese patent application laid-open No. 2017-96879
Patent document 2: japanese patent laid-open No. 2001-41867
Patent document 3: japanese patent laid-open No. 2019-512079
Patent document 4: japanese patent laid-open No. 2015-161543
Disclosure of Invention
In the test methods described in patent documents 1 and 2, although the strength test is performed by applying pressure to the columnar honeycomb structure in practice, the amount of work required for the test is still large, and the test time is also liable to be long. In addition, damage to the product is also possible. Patent document 3 discloses a method of predicting the isostatic fracture strength in a noncontact manner, but requires complicated simulation and the prediction accuracy is not known.
In patent document 4, an image analysis device is used to examine the presence or absence of a deformation defect in a part of cells included in a columnar honeycomb structure, and thereby calculate the proportion of cells in which the cell deformation defect occurs in a measurement cell. However, it is unknown what kind of relationship exists between the deformation defect of a part of the cells and the strength of the columnar honeycomb structure, and it is not suggested to estimate the strength of the columnar honeycomb structure from the deformation defect of a part of the cells.
The present invention has been made in view of the above-described circumstances, and an object of one embodiment is to provide a method for inspecting a columnar honeycomb formed body, which can be performed in a nondestructive manner and can be used instead of before or after firing for strength inspection.
The inventors of the present invention have made intensive studies to solve the above problems, and as a result, have found that the number of cells having an abnormal-sized opening among a plurality of cells included in a columnar ceramic molded body before firing or after firing and the strength of the columnar honeycomb molded body after firing show a clear correlation. The present invention has been made based on this knowledge, and will be exemplified below.
[1] A method for inspecting a columnar honeycomb molded body before firing, the columnar honeycomb molded body before firing having a columnar honeycomb structure portion having an outer peripheral side wall and partition walls disposed on an inner peripheral side of the outer peripheral side wall and partitioning a plurality of cells forming flow paths from a first bottom surface to a second bottom surface,
the method is characterized by comprising the following steps:
a step a1 of capturing, with a camera, at least one of a first bottom surface and a second bottom surface of the columnar honeycomb formed body before firing to generate an image of at least one of the first bottom surface and the second bottom surface;
a step b1 of measuring the sizes of the openings of the plurality of compartments in the image generated in the step a 1; and
and a step c1 of determining abnormal cells having openings with sizes deviating from a predetermined allowable range from among the plurality of cells based on the measurement result of the step b1, and counting the number of abnormal cells.
[2] The method according to [1], wherein,
the size of the openings of the plurality of compartments is based on the diameter of the largest circle that can be accommodated within the opening of each compartment, respectively.
[3] The method according to [1] or [2], characterized in that,
the method further includes a step d1 of estimating the strength of the columnar honeycomb molded body after firing under a predetermined condition from the number of abnormal cells measured in the step c1 by using a correlation between the number of abnormal cells obtained in advance for the other plurality of columnar honeycomb molded bodies having the same size and the same composition as the columnar honeycomb molded body before firing and the strength of the other plurality of columnar honeycomb molded bodies after firing under the predetermined condition.
[4] The method according to [3], wherein,
as the correlation, a determination coefficient (R 2 ) Is a correlation of 0.6 or more.
[5] The method according to [3] or [4], characterized in that,
the strength is the isostatic fracture strength.
[6] A method for inspecting a post-fired columnar honeycomb molded body having a columnar honeycomb structure portion having an outer peripheral side wall and partition walls disposed on the inner peripheral side of the outer peripheral side wall and partitioning a plurality of cells forming flow paths from a first bottom surface to a second bottom surface,
The method is characterized by comprising the following steps:
a step a2 of photographing at least one of the first bottom surface and the second bottom surface of the fired columnar honeycomb formed body with a camera to generate an image of at least one of the first bottom surface and the second bottom surface;
a step b2 of measuring the sizes of the openings of the plurality of cells in the image generated in the step a 2; and
and a step c2 of determining abnormal cells having openings with a size deviating from a predetermined allowable range from among the plurality of cells based on the measurement result of the step b2, and counting the number of abnormal cells.
[7] The method according to [6], wherein,
the size of the openings of the plurality of compartments is based on the diameter of the largest circle that can be accommodated within the opening of each compartment, respectively.
[8] The method according to [6] or [7], characterized in that,
the method further includes a step d2 of estimating the strength of the fired columnar honeycomb molded body based on the number of abnormal cells measured in the step c2, using a correlation between the number of abnormal cells obtained in advance for the other columnar honeycomb molded bodies having the same size, the same composition, and the same firing conditions and the strength of the other columnar honeycomb molded bodies.
[9] The method according to [8], wherein,
as the correlation, a determination coefficient (R 2 ) Is a correlation of 0.6 or more.
[10] The method according to [8] or [9], characterized in that,
the strength is the isostatic fracture strength.
Effects of the invention
The method for inspecting a columnar honeycomb formed body before or after firing according to one embodiment of the present invention can be performed in a nondestructive manner without applying a load to the columnar honeycomb formed body, and therefore, the possibility of damage to the columnar honeycomb formed body is extremely low. In addition, since the inspection method according to the present embodiment can replace the intensity inspection, it is not necessary to perform an additional intensity inspection. Based on the results obtained by the inspection method according to the present embodiment, the strength of the post-fired columnar honeycomb formed body can be estimated.
In the case of carrying out the inspection according to one embodiment of the present invention on the columnar honeycomb molded body before or after firing, the molded body that fails the inspection can be reused as a molding raw material. In particular, by performing the inspection according to one embodiment of the present invention on the columnar honeycomb molded body before firing, the strength inspection after firing can be replaced, and thus, the cost and time required for firing can be saved. In addition, if the molded article is before firing, it is easy to reuse the molded article that fails to be inspected as a molding material.
Drawings
Fig. 1 is a perspective view schematically showing a wall-penetrating columnar ceramic molded body.
Fig. 2 is a schematic cross-sectional view of the wall-penetrating columnar ceramic molded body as seen from a direction orthogonal to a direction in which the cells extend.
Fig. 3 is a perspective view schematically showing a columnar ceramic molded body of a wall flow type.
FIG. 4 is a schematic cross-sectional view of a columnar ceramic molded body of a wall flow pattern viewed from a direction orthogonal to a direction in which the cells extend.
FIG. 5 shows a result of plotting the relationship between the number of deformed cells of the columnar honeycomb molded body before firing and the isostatic fracture strength of the columnar honeycomb molded body after firing, which is related to test example 1, and a linear regression equation obtained by the least square method, and a determination coefficient (R 2 ) Together shown.
FIG. 6 shows a result of plotting the relationship between the number of deformed cells of the columnar honeycomb molded body before firing and the isostatic fracture strength of the columnar honeycomb molded body after firing, which is related to test example 2, and a linear regression equation obtained by the least square method, and a determination coefficient (R 2 ) Together shown.
Fig. 7 shows an example of a functional block diagram of the image analysis apparatus.
Symbol description
100. 200 … columnar honeycomb molding, 102, 202 … peripheral side wall, 104, 204 … first bottom surface, 106, 206 … second bottom surface, 108, 208a, 208b … compartment, 112, 212 … partition wall, 209 … hole sealing portion, 300 … image analysis device, 301 … data storage portion, 302 … display portion, 303 … input portion, 304 … operation portion.
Detailed Description
Next, embodiments of the present invention will be described in detail with reference to the drawings. The present invention is not limited to the following embodiments, and it is to be understood that modifications and improvements of the design may be appropriately made based on the general knowledge of those skilled in the art without departing from the gist of the present invention.
< 1. Columnar honeycomb molded article >)
The method for inspecting a columnar honeycomb molded body according to the present invention may be performed on a columnar honeycomb molded body before or after firing. Generally, a columnar honeycomb formed body has a columnar honeycomb structure portion including an outer peripheral side wall and partition walls which are arranged on the inner peripheral side of the outer peripheral side wall and partition a plurality of cells forming flow paths from a first bottom surface to a second bottom surface.
Fig. 1 and 2 are schematic perspective and sectional views of a wall-penetrating cylindrical honeycomb molding (100) that can be used as an exhaust gas filter and/or a catalyst carrier for automobiles. The columnar honeycomb formed body (100) has a columnar honeycomb structure portion having an outer peripheral side wall (102) and partition walls (112), wherein the partition walls (112) are arranged on the inner peripheral side of the outer peripheral side wall (102) and divide and form a plurality of cells (108) forming fluid flow paths from a first bottom surface (104) to a second bottom surface (106). In the columnar honeycomb formed body (100), both ends of each cell (108) are open, and exhaust gas flowing into one cell (108) from the first bottom surface (104) is purified while passing through the cell, and flows out from the second bottom surface (106).
Fig. 3 and 4 are schematic perspective and cross-sectional views of a wall-flow type columnar honeycomb molded body (200) which can be applied as an exhaust gas filter and/or a catalyst carrier for an automobile. The columnar honeycomb formed body (200) has a columnar honeycomb structure portion having an outer peripheral side wall (202) and partition walls (212), wherein the partition walls (212) are arranged on the inner peripheral side of the outer peripheral side wall (202) and divide into a plurality of cells (208 a, 208 b) forming fluid flow paths from a first bottom surface (204) to a second bottom surface (206).
In a columnar honeycomb molded body (200), a plurality of cells (208 a, 208 b) can be classified into a plurality of first cells (208 a) and a plurality of second cells (208 b), wherein the first cells (208 a) are arranged on the inner side of an outer peripheral side wall (202), extend from a first bottom surface (204) to a second bottom surface (206), and the first bottom surface (204) is open and has a hole sealing portion (209) on the second bottom surface (206), the second cells (208 b) are arranged on the inner side of the outer peripheral side wall (202), extend from the first bottom surface (204) to the second bottom surface (206), and have a hole sealing portion (209) on the first bottom surface (204) and the second bottom surface (206) are open. In the columnar honeycomb formed body (200), the first cells (208 a) and the second cells (208 b) are alternately arranged adjacent to each other with the partition walls (212) interposed therebetween.
If exhaust gas containing soot is supplied to the first bottom surface 204 on the upstream side of the fired columnar honeycomb formed body 200, the exhaust gas is introduced into the first cells 208a, and proceeds downstream in the first cells 208 a. The first compartment (208 a) has a hole sealing portion (209) on the downstream side second bottom surface (206), and therefore, exhaust gas permeates through a porous partition wall (212) that partitions the first compartment (208 a) and the second compartment (208 b), and flows into the second compartment (208 b). Soot cannot pass through the partition wall (212), and is thus trapped and accumulated in the first compartment (208 a). After the soot is removed, the clean exhaust gas flowing into the second compartment (208 b) advances downstream in the second compartment (208 b), and flows out from the second bottom surface (206) on the downstream side.
The shape of the bottom surface of the columnar honeycomb molded body (100, 200) is not limited, and may be, for example, a curved shape such as a circle, an ellipse, a racetrack shape, or an oblong shape, a polygonal shape such as a triangle or a quadrangle, or other irregular shape. The bottom surfaces of the illustrated columnar honeycomb molded bodies (100, 200) are circular in shape and columnar as a whole.
The shape of the cells in a cross section perpendicular to the flow path direction of the cells is not limited, and is preferably quadrangular, hexagonal, octagonal, or a combination thereof. Among them, square and hexagonal are preferable. By setting the cell shape to the above-described shape, the pressure loss when the fluid flows into the columnar honeycomb formed body is reduced, and the catalyst is excellent in purification performance.
The cell density (number of cells per unit cross-sectional area) is not particularly limited, and may be, for example, 6 to 2000 cells/square inch (0.9 to 311 cells/cm) 2 ) More preferably 50 to 1000 compartments/square inch (7.8 to 155 compartments/cm) 2 ) Particularly preferably 100 to 600 cells/square inch (15.5 to 92.0 cells/cm) 2 ). The cell density is calculated by dividing the number of cells in the columnar honeycomb molded bodies (100, 200) by one bottom area of the columnar honeycomb molded bodies (100, 200) excluding the outer peripheral side walls.
In the columnar honeycomb molded body after firing, the partition walls may be porous. The porosity of the partition walls may be appropriately adjusted according to the application, but is preferably 40% or more, more preferably 50% or more, and still more preferably 60% or more from the viewpoint of suppressing the pressure loss of the fluid to a low level. In addition, from the viewpoint of securing strength of the honeycomb formed body after firing, the porosity of the partition walls is preferably 80% or less, more preferably 75% or less, and still more preferably 70% or less. By using a mercury porosimeter, according to JIS R1655:2003, the porosity was measured by mercury intrusion.
The thickness of the partition walls is preferably 150 μm or more, more preferably 170 μm or more, and even more preferably 190 μm or more, from the viewpoint of improving the strength of the columnar honeycomb molded body after firing and the collection efficiency in the filter application. In addition, the thickness of the partition wall is preferably 260 μm or less, more preferably 240 μm or less, and further preferably 220 μm or less from the viewpoint of suppressing pressure loss.
When the columnar honeycomb molded body (100, 200) is used as a catalyst carrier, a catalyst corresponding to the purpose may be applied to the surface of the partition walls (112, 212). The catalyst is not limited, and examples thereof include: an oxidation catalyst (DOC) for oxidizing and burning Hydrocarbons (HC) and carbon monoxide (CO) to raise the temperature of exhaust gas, a PM combustion catalyst for assisting PM combustion such as soot, an SCR catalyst and an NSR catalyst for removing nitrogen oxides (NOx), and a three-way catalyst capable of simultaneously removing Hydrocarbons (HC), carbon monoxide (CO), and nitrogen oxides (NOx). The catalyst may suitably contain, for example, noble metals (Pt, pd, rh, etc.), alkali metals (Li, na, K, cs, etc.), alkaline earth metals (Mg, ca, ba, sr, etc.), rare earth metals (Ce, sm, gd, nd, Y, la, pr, etc.), transition metals (Mn, fe, co, ni, cu, zn, sc, ti, zr, V, cr, etc.), etc.
< 2 > Process for producing columnar honeycomb molded article
The columnar honeycomb molded body can be produced by a known production method, and will be described below by way of example. First, a raw material composition containing a ceramic raw material, a dispersion medium, a pore-forming agent, and a binder is kneaded to form a green body, and then the green body is extruded and molded, and dried, whereby a columnar honeycomb molded body before firing can be produced. Additives such as dispersants may be blended as necessary in the raw material composition. In the extrusion molding, a die having a desired overall shape, cell shape, partition wall thickness, cell density, and the like may be used.
In the drying step, conventionally known drying methods such as hot air drying, microwave drying, dielectric drying, reduced pressure drying, vacuum drying, and freeze drying can be used. Among them, a drying method in which hot air drying and microwave drying or dielectric drying are combined is preferable in that the entire molded body can be dried rapidly and uniformly. After forming plugging portions at predetermined positions on both bottom surfaces of the dried honeycomb formed body, the plugging portions are dried, whereby plugging portions can be formed.
The ceramic raw material is a raw material that remains after firing of metal oxide, metal, or the like and constitutes a part of the skeleton of the post-fired columnar honeycomb molded body (columnar honeycomb structure) in the form of ceramic. The ceramic raw material may be provided in the form of, for example, a powder. Examples of the ceramic raw material include raw materials for obtaining ceramics such as cordierite, mullite, zircon, aluminum titanate, silicon carbide, silicon nitride, zirconia, spinel, indian stone, sapphirine, corundum, and titania. Specific examples thereof include, but are not limited to: silica, talc, alumina, kaolin, serpentine, pyrophyllite, brucite, boehmite, mullite, magnesite, aluminum hydroxide, etc. The ceramic raw material may be used alone or in combination of 1 or more than 2.
In the case of filter applications such as DPF and GPF, cordierite can be preferably used as the ceramic. In this case, as the ceramic raw material, a cordierite forming raw material may be used. The cordierite forming raw material is a raw material that becomes cordierite by firing. The cordierite raw material preferably contains alumina (Al 2 O 3 ) (comprising aluminum hydroxide fraction converted to aluminum oxide): 30 to 45 mass% of magnesium oxide (MgO): 11 to 17 mass% of silicon dioxide (SiO) 2 ): 42 to 57 mass% of chemical composition.
The dispersion medium may be water or a mixed solvent of water and an organic solvent such as alcohol, and water is particularly preferably used.
The pore-forming agent is not particularly limited as long as it becomes pores after firing, and examples thereof include: wheat flour, starch, foaming resin, water-absorbent resin, silica gel, carbon (for example, graphite), ceramic foam, polyethylene, polystyrene, polypropylene, nylon, polyester, acryl, phenol, etc. The pore-forming agent may be used alone or in combination of at least 2 kinds. From the viewpoint of improving the porosity of the honeycomb formed body after firing, the content of the pore-forming agent is preferably 0.5 parts by mass or more, more preferably 2 parts by mass or more, and still more preferably 3 parts by mass or more, relative to 100 parts by mass of the ceramic raw material. From the viewpoint of securing the strength of the honeycomb formed body after firing, the content of the pore-forming agent is preferably 10 parts by mass or less, more preferably 7 parts by mass or less, and still more preferably 4 parts by mass or less, relative to 100 parts by mass of the ceramic raw material.
Examples of the binder include organic binders such as methyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, and polyvinyl alcohol. Particularly, methylcellulose and hydroxypropyl methylcellulose are preferably used together. In addition, from the viewpoint of improving the strength of the honeycomb formed body before firing, the content of the binder is preferably 4 parts by mass or more, more preferably 5 parts by mass or more, and still more preferably 6 parts by mass or more, relative to 100 parts by mass of the ceramic raw material. From the viewpoint of suppressing cracking caused by abnormal heat generation in the firing step, the content of the binder is preferably 9 parts by mass or less, more preferably 8 parts by mass or less, and even more preferably 7 parts by mass or less, relative to 100 parts by mass of the ceramic raw material. The binder may be used alone or in combination of 1 or more than 2.
As the dispersant, ethylene glycol, dextrin, fatty acid soap, polyether polyol and the like can be used. The dispersant may be used alone or in combination of 1 or more than 2. The content of the dispersant is preferably 0 to 2 parts by mass relative to 100 parts by mass of the ceramic raw material.
The columnar honeycomb molded body can be formed such that both ends of all cells are open like the columnar honeycomb molded body (100). The columnar honeycomb molded body may have a cell structure in which one end of the cells is alternately plugged, as in the columnar honeycomb molded body (200). The method of sealing the bottom surface of the columnar honeycomb formed body is not particularly limited, and a known method can be used.
The material of the sealing portion is not particularly limited, and ceramic is preferable from the viewpoints of strength and heat resistance. The ceramic is preferably a ceramic containing at least 1 selected from the group consisting of cordierite, mullite, zircon, aluminum titanate, silicon carbide, silicon nitride, zirconia, spinel, indian, sapphirine, corundum, and titania. The sealing portion is preferably formed of a material containing 50 mass% or more of the ceramics in total, and more preferably formed of a material containing 80 mass% or more of the ceramics. In order to make the expansion ratio at the time of firing the honeycomb body uniform and to improve the durability, the plugging portion is further preferably made of the same material composition as the main body portion of the honeycomb formed body.
A method of forming the hole sealing portion will be described exemplarily. The sealing slurry is stored in a storage container in advance. Next, a mask having an opening at a portion corresponding to a compartment where a hole sealing portion is to be formed is stuck to one bottom surface. The bottom surface to which the mask is attached is immersed in a storage container, and the opening is filled with a sealing slurry, thereby forming a sealing portion. The other bottom surface may be formed with a hole sealing portion by the same method.
Degreasing and firing are performed on the columnar honeycomb molded body before firing, whereby a post-fired columnar honeycomb molded body (columnar honeycomb structure) can be produced. The conditions of the degreasing step and the firing step may be any known conditions depending on the material composition of the honeycomb formed body, and the specific conditions are exemplified below, although no particular explanation is required.
The degreasing process will be described. The combustion temperature of the adhesive is about 200 ℃, and the combustion temperature of the pore-forming agent is about 300-1000 ℃. Therefore, the degreasing step may be performed by heating the honeycomb formed body to a temperature in the range of about 200 to 1000 ℃. The heating time is not particularly limited, and is usually about 10 to 100 hours. The honeycomb formed body after the degreasing step is called a calcined body.
The firing step may be performed by heating the calcined body to 1350 to 1600 ℃ and holding the calcined body for 3 to 10 hours, for example, depending on the material composition of the honeycomb formed body.
< 3. Inspection method of columnar honeycomb molded article before or after firing >)
In accordance with one embodiment of the present invention,
a method for inspecting a columnar honeycomb molded body before firing, the columnar honeycomb molded body before firing having a columnar honeycomb structure portion having an outer peripheral side wall and partition walls disposed on an inner peripheral side of the outer peripheral side wall and partitioning a plurality of cells forming flow paths from a first bottom surface to a second bottom surface,
the method is characterized by comprising the following steps:
a step a1 of capturing, with a camera, at least one of a first bottom surface and a second bottom surface of the columnar honeycomb formed body before firing to generate an image of at least one of the first bottom surface and the second bottom surface;
A step b1 of measuring the sizes of the openings of the plurality of compartments in the image generated in the step a 1; and
and a step c1 of determining abnormal cells having openings with sizes deviating from a predetermined allowable range from among the plurality of cells based on the measurement result of the step b1, and counting the number of abnormal cells.
In accordance with a further embodiment of the present invention,
a method for inspecting a post-fired columnar honeycomb molded body having a columnar honeycomb structure portion having an outer peripheral side wall and partition walls disposed on the inner peripheral side of the outer peripheral side wall and partitioning a plurality of cells forming flow paths from a first bottom surface to a second bottom surface,
the method is characterized by comprising the following steps:
a step a2 of photographing at least one of the first bottom surface and the second bottom surface of the fired columnar honeycomb formed body with a camera to generate an image of at least one of the first bottom surface and the second bottom surface;
a step b2 of measuring the sizes of the openings of the plurality of cells in the image generated in the step a 2; and
And a step c2 of determining abnormal cells having openings with a size deviating from a predetermined allowable range from among the plurality of cells based on the measurement result of the step b2, and counting the number of abnormal cells.
As described above, the number of cells having an abnormal-sized opening and the strength of the columnar honeycomb molded body after firing show a clear correlation. Therefore, the strength of the post-fired columnar honeycomb molded body can be estimated based on the number of cells having an opening of an abnormal size.
Accordingly, the inspection method according to the present invention may further include a step d1 of estimating the strength of the columnar honeycomb molded body after firing the columnar honeycomb molded body before firing under a predetermined condition based on the number of abnormal cells measured in the step c1, using a correlation between the number of abnormal cells obtained in advance for the other plurality of columnar honeycomb molded bodies having the same size and the same composition as the columnar honeycomb molded body before firing and the strength of the other plurality of columnar honeycomb molded bodies after firing under the predetermined condition. Similarly, the inspection method according to the present invention further includes a step d2 of estimating the strength of the fired columnar honeycomb molded body based on the number of abnormal cells measured in the step c2, using a correlation between the number of abnormal cells obtained in advance for the other columnar honeycomb molded bodies having the same size and the same composition and manufactured under the same firing conditions as the fired columnar honeycomb molded body and the strength of the other columnar honeycomb molded bodies.
(Process a1 or Process a 2)
In step a1 or step a2, at least one of the first bottom surface and the second bottom surface of the columnar honeycomb formed body before or after firing is photographed by a camera, and an image of at least one of the first bottom surface and the second bottom surface is generated. In order to improve the inspection accuracy, it is preferable to generate images of both the first bottom surface and the second bottom surface. In particular, in the case of a columnar honeycomb molded body having a plugged portion, cells having a plugged portion have cells in which the size of an opening cannot be measured even if one bottom surface is photographed, and therefore, it is preferable to generate images on both bottom surfaces as inspection targets.
When the first bottom surface or the second bottom surface is photographed by the camera, the entire first bottom surface or the second bottom surface is preferably photographed. This is to inspect substantially all of the compartments that can be seen from either the first or second bottom surface. However, a part of the cells may not be an object of examination, but may be excluded from the object of photographing. The partial compartments refer to: a compartment located at the outermost periphery and at least a portion of which is defined by the peripheral sidewall. Since a part of the outline of the partial cell is formed by the peripheral side wall, the shape is different from the cell other than the partial cell (hereinafter also referred to as "normal cell") and the area is smaller than the normal cell. In addition, the number of partial compartments is particularly small compared to the usual compartments. Therefore, the abnormality of part of the cells has less influence on the strength of the post-firing columnar honeycomb molded body. Further, since some compartments are smaller than the normal compartments, if it is desired to separate from the normal compartments to detect an abnormality, it is necessary to separately set the determination conditions for the abnormal compartments, and thus the inspection is complicated.
On the other hand, in general, the number of cells is excessively large, and the abnormality thereof greatly affects the strength of the columnar honeycomb molded body after firing. Therefore, it is preferable to set 90% or more, preferably 95% or more, more preferably all of the cells to be inspected.
The photographing by the camera is performed from a direction perpendicular to the first bottom surface or the second bottom surface, which is desirable in terms of improving inspection accuracy. The camera may be an area camera (area camera) or a line camera (line camera), but is preferably an area camera for reasons such as high imaging speed, wide illumination range, and capability of reducing the size of the device. From the viewpoint of improving inspection accuracy, a camera with high pixel resolution is preferably used. Specifically, in the camera, if the normal opening area of the compartment is considered, the resolution of the pixel is preferably 40 μm or less per pixel in both the vertical direction and the horizontal direction, more preferably 25 μm or less per pixel, and may be, for example, 1 to 40 μm per pixel.
(Process b1 or Process b 2)
In step b1 or step b2, the sizes of the openings of the plurality of cells are measured in the image generated in step a1 or step a 2. The measurement of the opening size may be performed by an inspector based on an image, but since the number of compartments to be inspected is large, it is preferable to perform the automatic measurement by using an image analysis device. Hereinafter, an example of a measurement procedure using the image analysis apparatus will be described. There are various parameters indicating the opening sizes of the respective compartments, and examples thereof include: the opening area of each compartment, the diameter of the largest circle that can be accommodated in the opening of each compartment, and the like. Among them, the maximum circle that can be accommodated in the opening of each compartment is preferable because the correlation between the diameter and the strength is high.
(Process c1 or Process c 2)
Based on the measurement results in step b1 or step b2, an abnormal cell having an opening with a size deviating from a predetermined allowable range is determined from among the plurality of cells, and the number of abnormal cells is counted. The abnormal cells may be measured by an inspector, but from the viewpoint of shortening the time, it is preferable to automatically measure the abnormal cells by using an image analysis device. Hereinafter, an example of a measurement procedure using the image analysis device will be described.
In the case where the inspection method according to the present embodiment is intended to be implemented instead of the strength inspection, the height of the correlation is changed according to the setting of the allowable range, and therefore, the allowable range is preferably set as a condition under which a high correlation between the number of abnormal cells and the strength of the post-fired columnar honeycomb structure can be confirmed. Specifically, when a columnar honeycomb molded body before firing is to be inspected, a correlation between the number of abnormal cells obtained in advance for another plurality of columnar honeycomb molded bodies having the same size and the same composition as those of the columnar honeycomb molded body before firing and the strength of the other plurality of columnar honeycomb molded bodies after firing under a predetermined condition is obtained, Determining coefficient (R) 2 ) Preferably 0.6 or more, typically 0.6 to 0.8, more typically 0.6 to 0.7. In the case of taking a post-fired columnar honeycomb molded body as an inspection object, a correlation between the number of abnormal cells and the strength of other columnar honeycomb molded bodies obtained in advance for the other columnar honeycomb molded bodies of the same size, the same composition and the same firing conditions as the post-fired columnar honeycomb molded body is calculated, and a determination coefficient (R 2 ) Preferably 0.6 or more, typically 0.6 to 0.8, more typically 0.6 to 0.7.
As a specific example of the allowable range, when the diameter of the largest circle that can be accommodated in the opening is set to the size of the opening, a compartment having a ratio of the size of the opening to the size of the opening of the designed compartment of 93% or more may be used as the normal compartment.
(step d1 or step d 2)
In the step d1, the strength of the columnar honeycomb molded body after firing the columnar honeycomb molded body before firing under a predetermined condition is estimated based on the number of abnormal cells measured in the step c1, using a correlation between the number of abnormal cells obtained in advance for the other plurality of columnar honeycomb molded bodies of the same size and the same composition as the columnar honeycomb molded body before firing and the strength of the other plurality of columnar honeycomb molded bodies after firing under the predetermined condition.
In the step d2, the strength of the fired columnar honeycomb molded body is estimated based on the number of abnormal cells measured in the step c2, using a correlation between the number of abnormal cells obtained in advance for other columnar honeycomb molded bodies having the same size and the same composition as the fired columnar honeycomb molded body and manufactured under the same firing conditions and the strength of the other columnar honeycomb molded bodies.
From the viewpoint of improving the estimation accuracy of the intensity, the correlation used in the step d1 or the step d2 is preferably a determination coefficient (R 2 ) Is a correlation of 0.6 or more. Excellent (excellent)Selecting a coefficient of determination (R 2 ) Higher, typically 0.6 to 0.8, more typically 0.6 to 0.7, may be used.
There are various parameters showing the strength of the columnar honeycomb molded body, and examples thereof include isostatic fracture strength and compressive strength. Among them, the correlation between the isostatic fracture strength and the opening size of the compartment is high, and therefore, the estimation accuracy is also high.
Determining coefficient (R) 2 ) And taking a value of 0 to 1 for the parameter representing the accuracy scale of the regression equation. Regarding the strength of the columnar honeycomb molded body and the number of abnormal cells, it can be said that: the closer the determination coefficient to 1 when the regression equation is obtained from the measured data, the higher the correlation between the two is, and the intensity can be estimated with high accuracy from the number of abnormal cells.
Determining coefficient (R) 2 ) The solution is performed using the following equation.
[ math 1 ]
(x i ，y i ) As measured data
For data deduced from regression equations
For the average value obtained from the whole data
n is the number of data
(image analysis device)
Fig. 7 shows an example of a functional block diagram of the image analysis device (300). An image analysis device (300) is provided with: a data storage unit (301), a display unit (302), an input unit (303), and a calculation unit (304).
The data storage unit (301) may be configured from, for example, a semiconductor memory, and can store image data of at least one of the first bottom surface and the second bottom surface of the columnar honeycomb molded body produced by the camera. In addition, an allowable range regarding the opening size of the compartment for discriminating an abnormal compartment can be stored.
The input unit (303) may be configured by, for example, a keyboard, a touch panel, a keypad, a mouse, or the like, and the inspector may issue a start instruction for performing image analysis on a desired image representing the first bottom surface or the second bottom surface of the columnar honeycomb formed body via the input unit (303).
The display unit (302) may be configured by a display device such as a liquid crystal display or an organic EL display, and is capable of displaying the image data stored in the data storage unit (301). In addition, the result of the image analysis can be displayed.
The arithmetic unit (304) may be constituted by CPU (Central Processing Unit), MPU (Micro Processing Unit), or the like, for example. When receiving an instruction to start image analysis from an input unit (303), an arithmetic unit (304) can execute image analysis based on the image data stored in the data storage unit (301) to determine an abnormal compartment and measure the abnormal compartment.
For image analysis, in one embodiment, the following steps are performed: the method includes a step of performing image processing on an image of at least one of a first bottom surface and a second bottom surface of a columnar honeycomb formed body captured by a camera, a step of measuring the opening sizes of a plurality of cells included in at least one of the first bottom surface and the second bottom surface based on the image of at least one of the first bottom surface and the second bottom surface obtained by the image processing step, and a step of determining abnormal cells having openings with a size that deviates from a predetermined allowable range from among the plurality of cells based on the measurement result of the step of measuring the opening sizes, and measuring the number of the abnormal cells.
In order to easily measure the size of the opening, in the image processing step, the computing unit (304) preferably performs image processing including:
Binarizing an image of at least one of the first bottom surface and the second bottom surface of the columnar honeycomb formed body, based on a predetermined threshold value of brightness, the inner peripheral side of the outer peripheral side wall into two regions, namely, an opening region of the cell, a partition region and an outer peripheral side wall region;
a step of discriminating the outer side of the region, which is obtained by shifting the outline of the outer surface forming the outer peripheral side wall to the inner side by a predetermined threshold value, into an outer peripheral side wall region after the binarization processing, and determining a partition wall region;
smoothing the determined partition wall region by averaging and filtering;
a skeletonizing process of extracting a core wire of the partition wall region from the partition wall region after the smoothing process; and
and a swelling treatment of the core wire extracted by the skeletonizing treatment.
The threshold value in the binarization process may be set from the viewpoint of distinguishing and identifying the opening region from the partition wall region and the outer peripheral side wall region. For example, when the background is black, the threshold value may be set in the range of 30 to 100, preferably 50 to 80 when the white-to-black degree of the pixel is 0 to 255. By performing the binarization processing, the partition wall portion and the opening portion can be clearly divided, and an advantage of facilitating image analysis can be obtained.
The smoothing processing may employ an averaging filter that updates the value of the pixel in the central portion of the region with an average value of the pixel values of the region determined by, for example, 9 (vertical 3×horizontal 3) or 25 (vertical 5×horizontal 5) pixels. Since noise is removed by performing the smoothing process, the partition wall portion can be recognized more clearly when performing the image processing described later, and the advantage of improving the inspection accuracy can be obtained.
In the skeletonizing process, for example, circles having diameters corresponding to the thicknesses of the partition walls are adjacent to each other in the direction in which the partition walls extend, and are arranged in series in the partition wall region, and center pixels of the circles are connected to each other, whereby the core line can be extracted. By performing the skeletonizing process, the center line of the partition wall can be recognized, and therefore, the linearity of the partition wall can be recognized clearly, and the advantage of improving the inspection accuracy can be obtained.
The swelling treatment is preferably performed in a range of, for example, 20 μm to 200 μm until the thickness of the partition wall reaches a predetermined number of pixels. However, if the swelling treatment is excessively performed, the cell opening size greatly changes, and therefore, it is more preferable to perform the treatment by swelling the core wire to a thickness of the partition wall corresponding to the design value of the columnar honeycomb molded body to be inspected. Consider that: by performing the expansion process, the linearity of the partition wall can be emphasized, and the inspection close to the actual state can be performed, so that the inspection accuracy is improved.
After the image processing, an arithmetic unit (304) corrects the opening area of the cells by using the expanded core line as a partition area, and measures the opening sizes of the cells based on the corrected opening area of the cells. As mentioned above, it is preferred to exclude a part of the compartments from the compartments measuring the size of the opening.
(quality inspection)
According to one embodiment of the present invention, there is provided a method for performing quality inspection of a columnar honeycomb formed body before or after firing based on the number of abnormal cells measured by the above-described inspection method. For example, a linear regression equation or a nonlinear regression equation showing the correlation between the number of abnormal cells and the strength of the post-firing columnar honeycomb molded body is derived based on the correlation between the number of abnormal cells and the strength of the post-firing columnar honeycomb molded body, and the number of allowable abnormal cells ("allowable abnormal cells") is calculated in advance based on the strength required for the post-firing columnar honeycomb molded body. Then, in the quality inspection, the number of abnormal cells counted by the inspection method described above is compared with the allowable number of abnormal cells. For example, if the number of abnormal cells counted exceeds the allowable number of abnormal cells, the inspected columnar honeycomb molded body is determined to be defective, and if the number of abnormal cells counted is equal to or less than the allowable number of abnormal cells, the columnar honeycomb molded body may be determined to be acceptable.
According to another embodiment of the present invention, there is provided a method for inspecting the quality of a columnar honeycomb molded body before or after firing based on the strength estimated in the inspection method. For example, in the quality inspection, if the estimated strength is lower than the strength required for the post-fired columnar honeycomb molded body, the inspected columnar honeycomb molded body is determined to be defective, and if the estimated strength is equal to or higher than the required strength, the inspected columnar honeycomb molded body is determined to be acceptable.
The pass/fail determination by the quality inspection may be performed by an inspector based on the number of abnormal cells or the estimated intensity, or may be performed by the image analysis device (300). In this case, the data storage unit (301) stores information on the allowable number of abnormal cells and/or the strength required for the post-firing columnar honeycomb molded body. The calculation unit (304) may determine whether the number of abnormal cells counted is acceptable or unacceptable based on the information, or whether the estimated strength is acceptable or unacceptable based on the strength required for the post-firing columnar honeycomb molded body. The image analysis device (300) may be configured such that the result of the match/fail determination is displayed on the display unit (302).
Examples
Test example 1 >
(1. Production of columnar honeycomb molded article)
6 parts by mass of a pore-forming agent, 35 parts by mass of a dispersion medium, 6 parts by mass of an organic binder and 0.5 part by mass of a dispersant were added to 100 parts by mass of a cordierite forming raw material, and the resultant mixture was mixed and kneaded to prepare a clay. As cordierite forming raw materials, alumina, aluminum hydroxide, kaolin, talc, and silica are used. Water is used as a dispersion medium, coke having an average particle diameter of 1 to 10 μm is used as a pore-forming agent, hydroxypropyl methylcellulose is used as an organic binder, and ethylene glycol is used as a dispersing agent.
The clay was put into an extrusion molding machine and extrusion molded, whereby a columnar honeycomb molded body was obtained. After dielectric drying and hot air drying of the obtained honeycomb formed body, both bottom surfaces were cut into predetermined dimensions to obtain a number of dried cylindrical honeycomb formed bodies required for the following test.
The specifications of the columnar honeycomb molded body were as follows.
Overall shape: cylindrical with diameter of 142mm x height of 98mm
Cell shape in a cross section perpendicular to the flow path direction of a normal cell: square shape
Design dimensions of the opening in a cross section perpendicular to the flow path direction of the usual compartment: 1.032 mm. Times.1.032 mm (the largest circle that can be accommodated in the opening of a normal compartment in design has a diameter of 1.032 mm)
Cell density (number of cells per unit cross-sectional area): 93 compartment/cm 2
Thickness of partition wall design: 70 μm
(2. Measurement of the size of the opening of the Compartment)
The cell opening sizes of the obtained columnar honeycomb molded bodies (sample Nos. 1-1 to 1-36) were measured in accordance with the following procedure. One bottom surface of each columnar honeycomb molded body was photographed from a direction perpendicular to the bottom surface by a camera (pixel resolution 0.01174 mm/pixel in the vertical direction, pixel resolution 0.01174 mm/pixel in the horizontal direction), and an image of the bottom surface was generated. The image was analyzed by an image analysis device (HALCON, MVTec corporation) to measure the opening sizes of all cells except for a part of the cells. The results are shown in Table 1.
In the image analysis, the following image processing is performed by the image analysis device.
Binarization processing: in the image of the bottom surface, the inner peripheral side of the peripheral side wall is divided into two regions (50 threshold value: background black, white-black level of the pixel is 0 to 255 level) of an opening region and a partition region of the compartment based on a predetermined threshold value of brightness
Smoothing processing: for the partition area after the binarization processing, averaging filtering is performed to update the average value of pixel values of the area determined by 9 (vertical 3×horizontal 3) pixels
Skeletonizing treatment: extracting core wire of partition wall region from partition wall region after smoothing treatment
Expansion treatment: expanding the core wire extracted by skeletonizing to a thickness of the design of the partition wall
Next, based on the image of the bottom surface after the image processing, the opening sizes of all the compartments except for a part of the compartments included in the bottom surface are measured by an image analysis device. As a parameter of the opening size, the diameter of the largest circle that can be accommodated in the opening of each compartment is used.
(3. Firing of columnar honeycomb molded article)
Then, each columnar honeycomb formed body is degreased under the atmosphere at about 200 to 1000 ℃, and then heated to 1350 to 1600 ℃ and fired under firing conditions of about 3 to 10 hours.
(4. Measurement of isostatic fracture Strength)
Based on the automobile standards (JASO M505-87) issued by the society of automotive technology, the isostatic fracture strength (isostatic value) of each columnar honeycomb molded body (sample No.1-1 to 1-36) after firing was measured. The results are shown in Table 1. The interpretation method of the table is described. The opening size of the compartment (compartment opening size) is determined to the size of half the pixel. The sample No.1-1 had an equivalent loss of 2.12MPa. The sample for No.1-1 is shown: the number of compartments with a maximum circle diameter of 38.0pixel (0.892 mm) or less is 1, and the number of compartments with an opening size of 38.5pixel (0.904 mm) or less is 4. Other opening sizes are also the same. In the table, "R square" is: a determination coefficient (R 2 ). The compartments with opening sizes exceeding 43.5 pixels (1.021 mm) were hardly seen in any of the samples, and are not shown in the table.
In FIG. 5, for test example 1, the relationship between the number of deformed cells of the columnar honeycomb molded body before firing and the isostatic fracture strength of the columnar honeycomb molded body after firing was plotted with a linear regression equation and a determination coefficient (R) obtained by the least square method when the allowable range of the normal cells was set to 0.963mm to 1.021mm 2 ) Together shown.
From the above results, it was found that if the allowable range of the normal compartments is set to 0.963mm to 1.021mm, the coefficient of determination (R 2 ) 0.6091, the two have higher correlation. Thus, it can be seen that: based on the number of abnormal cells of the columnar honeycomb molded body before firing, the isostatic fracture strength of the columnar honeycomb molded body after firing can be estimated.
TABLE 1
Test example 2 >
(1. Production of columnar honeycomb molded article)
A dried cylindrical honeycomb molded body was produced in the same manner as in test example 1, except that the entire shape was changed to a cylindrical honeycomb molded body having a diameter of 192mm×a height of 120mm, according to the requirements of the following test.
(2. Measurement of the size of the opening of the Compartment)
The opening sizes of all cells except for a part of the cells were measured for each of the obtained columnar honeycomb molded bodies (sample Nos. 2-1 to 2-47) in the same manner as in test example 1. The results are shown in Table 2. The compartments with opening sizes exceeding 43.5 pixels (1.021 mm) were hardly seen in any of the samples, and are not shown in the table.
(3. Firing of columnar honeycomb molded article)
Then, each columnar honeycomb formed body is degreased under the atmosphere at about 200 to 1000 ℃, and then heated to 1350 to 1600 ℃ and fired under firing conditions of about 3 to 10 hours.
(4. Measurement of isostatic fracture Strength)
The isostatic fracture strength of each columnar honeycomb molded body (sample No.2-1 to 2-47) after firing was measured in the same manner as in test example 1. The results are shown in Table 2. In FIG. 6, in test example 2, the allowable range of the normal compartment is set to 0.963mm to 1.02The relationship between the number of deformation cells of the columnar honeycomb molded body before firing at 1mm and the isostatic fracture strength of the columnar honeycomb molded body after firing was plotted with a linear regression equation obtained by the least square method and a determination coefficient (R 2 ) Together shown.
From the above results, it was found that if the allowable range of the normal compartments is set to 0.963mm to 1.021mm, the coefficient of determination (R 2 ) 0.6510, the two have higher correlation. Thus, it can be seen that: based on the number of abnormal cells of the columnar honeycomb molded body before firing, the isostatic fracture strength of the columnar honeycomb molded body after firing can be estimated.
TABLE 2
Since the cell sizes are not substantially different after firing, the isostatic fracture strength of the post-firing columnar honeycomb molded body may be estimated based on the number of abnormal cells of the post-firing columnar honeycomb molded body.
Claims (8)
1. A method for inspecting a columnar honeycomb molded body before firing, the columnar honeycomb molded body before firing having a columnar honeycomb structure portion having an outer peripheral side wall and partition walls disposed on an inner peripheral side of the outer peripheral side wall and partitioning a plurality of cells forming flow paths from a first bottom surface to a second bottom surface,
the method is characterized by comprising the following steps:
a step a1 of capturing, with a camera, at least one of a first bottom surface and a second bottom surface of the columnar honeycomb formed body before firing to generate an image of at least one of the first bottom surface and the second bottom surface;
A step b1 of measuring the sizes of the openings of the plurality of compartments in the image generated in the step a 1; and
a step c1 of determining an abnormal compartment having an opening with a size deviating from a predetermined allowable range from among the plurality of compartments based on the measurement result of the step b1, counting the number of abnormal compartments,
and a step d1 of estimating the strength of the columnar honeycomb molded body after firing under a predetermined condition based on the number of abnormal cells measured in the step c1 by using a correlation between the number of abnormal cells obtained in advance for the other plurality of columnar honeycomb molded bodies having the same size and the same composition as the columnar honeycomb molded body before firing and the strength of the other plurality of columnar honeycomb molded bodies after firing under the predetermined condition.
2. The method of claim 1, wherein the step of determining the position of the substrate comprises,
the size of the openings of the plurality of compartments is based on the diameter of the largest circle that can be accommodated within the opening of each compartment, respectively.
3. The method of claim 1, wherein the step of determining the position of the substrate comprises,
as the correlation, a determination coefficient R in solving a linear regression equation is used 2 Is a correlation of 0.6 or more.
4. The method of claim 1, wherein the step of determining the position of the substrate comprises,
the strength is the isostatic fracture strength.
5. A method for inspecting a post-fired columnar honeycomb molded body having a columnar honeycomb structure portion having an outer peripheral side wall and partition walls disposed on the inner peripheral side of the outer peripheral side wall and partitioning a plurality of cells forming flow paths from a first bottom surface to a second bottom surface,
the method is characterized by comprising the following steps:
a step a2 of photographing at least one of the first bottom surface and the second bottom surface of the fired columnar honeycomb formed body with a camera to generate an image of at least one of the first bottom surface and the second bottom surface;
a step b2 of measuring the sizes of the openings of the plurality of cells in the image generated in the step a 2; and
a step c2 of determining an abnormal compartment having an opening with a size deviating from a predetermined allowable range from among the plurality of compartments based on the measurement result of the step b2, counting the number of abnormal compartments,
and a step d2 of estimating the strength of the fired columnar honeycomb molded body based on the number of abnormal cells measured in the step c2, using a correlation between the number of abnormal cells obtained in advance for other columnar honeycomb molded bodies having the same size and the same composition as the fired columnar honeycomb molded body and manufactured under the same firing conditions and the strength of the other columnar honeycomb molded bodies.
6. The method of claim 5, wherein the step of determining the position of the probe is performed,
the size of the openings of the plurality of compartments is based on the diameter of the largest circle that can be accommodated within the opening of each compartment, respectively.
7. The method of claim 5, wherein the step of determining the position of the probe is performed,
as the correlation, a determination coefficient R in solving a linear regression equation is used 2 Is a correlation of 0.6 or more.
8. The method of claim 5, wherein the step of determining the position of the probe is performed,
the strength is the isostatic fracture strength.
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| JP2020040295A JP7213198B2 (en) | 2020-03-09 | 2020-03-09 | Method for inspecting columnar honeycomb molded body before or after firing |
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| JP6530680B2 (en) * | 2015-09-02 | 2019-06-12 | 日本碍子株式会社 | Plugged honeycomb structure and plugged honeycomb segment |
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| JP6881337B2 (en) * | 2018-01-30 | 2021-06-02 | 株式会社デンソー | Honeycomb structure and mold |
| JP7035567B2 (en) * | 2018-01-30 | 2022-03-15 | 株式会社デンソー | Honeycomb structure and mold |
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| JP2002257736A (en) * | 2001-03-02 | 2002-09-11 | Ngk Insulators Ltd | Method and device for inspecting end face of honeycomb structure |
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| US20210279849A1 (en) | 2021-09-09 |
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